US20090197026A1 - Composition for treating glass-ceramic or glass to improve mechanical strength through curing of surface defects, treatment methods - Google Patents

Composition for treating glass-ceramic or glass to improve mechanical strength through curing of surface defects, treatment methods Download PDF

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US20090197026A1
US20090197026A1 US11/630,772 US63077205A US2009197026A1 US 20090197026 A1 US20090197026 A1 US 20090197026A1 US 63077205 A US63077205 A US 63077205A US 2009197026 A1 US2009197026 A1 US 2009197026A1
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Prior art keywords
composition
glass
constituent
ceramic
coating
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US11/630,772
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English (en)
Inventor
Pablo Vilato
Marie-Héléne Rouillon
Caroline Faillat
Sophie Besson
Stéphane Lohou
Olivier Gaume
Didier Le Couviour
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Eurokera SNC
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Eurokera SNC
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Assigned to EUROKERA S.N.C. reassignment EUROKERA S.N.C. ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: BESSON, SOPHIE, FAILLAT, CAROLINE, GAUME, OLIVIER, LE COUVIOUR, DIDIER, LOHOU, STEPHANE, ROUILLON, MARIE-HELENE, VILATO, PABLO
Publication of US20090197026A1 publication Critical patent/US20090197026A1/en
Abandoned legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/28—Surface treatment of glass, not in the form of fibres or filaments, by coating with organic material
    • C03C17/30—Surface treatment of glass, not in the form of fibres or filaments, by coating with organic material with silicon-containing compounds
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/22—Surface treatment of glass, not in the form of fibres or filaments, by coating with other inorganic material
    • C03C17/23—Oxides
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C25/00—Surface treatment of fibres or filaments made from glass, minerals or slags
    • C03C25/10—Coating
    • C03C25/104—Coating to obtain optical fibres
    • C03C25/106—Single coatings
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C25/00—Surface treatment of fibres or filaments made from glass, minerals or slags
    • C03C25/10—Coating
    • C03C25/24—Coatings containing organic materials
    • C03C25/40—Organo-silicon compounds
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/13—Hollow or container type article [e.g., tube, vase, etc.]
    • Y10T428/131—Glass, ceramic, or sintered, fused, fired, or calcined metal oxide or metal carbide containing [e.g., porcelain, brick, cement, etc.]
    • Y10T428/1317—Multilayer [continuous layer]
    • Y10T428/1321—Polymer or resin containing [i.e., natural or synthetic]
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
    • Y10T428/2913—Rod, strand, filament or fiber
    • Y10T428/2933—Coated or with bond, impregnation or core
    • Y10T428/2938—Coating on discrete and individual rods, strands or filaments
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/31504—Composite [nonstructural laminate]
    • Y10T428/31551—Of polyamidoester [polyurethane, polyisocyanate, polycarbamate, etc.]
    • Y10T428/31616—Next to polyester [e.g., alkyd]
    • Y10T428/3162—Cross-linked polyester [e.g., glycerol maleate-styrene, etc.]

Definitions

  • the present invention relates to a composition for treating a glass-ceramic, especially in plate form, a glass, in particular flat glass or hollowware (bottles, flasks, etc.), or glass in the form of fibers, in order to improve the mechanical strength of said glass by healing surface defects thereon.
  • the invention also relates to the corresponding treatment methods and to the glass thus treated.
  • the surface temperature of the glass during application of the treatment agent rises to at least 30° C., being especially between 30 and 150° C. Through this treatment, the resistance to prolonged use of the containers is improved.
  • U.S. Pat. No. 6,403,175 B1 describes an agent for the cold treatment of hollowware containers for their surface reinforcement.
  • This water-based agent contains at least the following components: a trialkoxysilane, a dialkoxysilane and/or a tetraalkoxysilane, their hydrolysis products and/or their condensation products; a water-soluble mixture of a polyol and a crosslinking agent for the polyol, the layer of cold treatment agent thus applied then being crosslinked over a temperature range between 100 and 350° C.
  • the subject of the present invention is therefore a composition for treating the surface of a glass-ceramic, especially in plate form, or glass, in particular flat glass or hollowware, or glass in the form of fibers, said composition being able to be applied as a thin coating to said glass-ceramic or said glass, characterized in that it comprises, in aqueous medium, the following constituents (A) and (B):
  • the alkyl residue for R is especially a linear or branched C 1 -C 8 alkyl residue.
  • the functional groups f (A) and f (B) may especially be chosen from —NH 2 , —NH—, epoxy, vinyl, (meth)acrylate, isocyanate and alcohol functional groups.
  • the functional groups f (A) and f (B) of the constituents (A) and (B), respectively, may be chosen from the families indicated in the table below, with the thin coating being formed by UV-activated or thermally activated curing:
  • the functional groups f (A) of constituent (A) are —NH 2 and/or —NH-functional groups and the functional groups f (B) of constituent (B) are epoxy functional groups
  • the ratio of the number of —NH-functional groups of constituent (A) to the number of epoxy functional groups is between 0.3/1 and 3/1, limits inclusive, especially between 0.5/1 and 1.5/1, limits inclusive.
  • composition according to the invention which comprises 3-aminopropyltriethoxysilane as constituent (A) and glycidoxypropylmethyldiethoxysilane as constituent (B), but after being advantageously introduced in the prehydrolyzed state.
  • constituents (A) and (B), at least one of which includes at least one —SiOR functional group undergo hydrolysis of the —SiOR functional group or groups into —SiOH over a relatively long time period after the contacting with water.
  • an acid such as hydrochloric acid or acetic acid, has to be added in order to catalyze the hydrolysis.
  • the condensation of the —SiOH functional groups into —SiO—Si— groups may even start at room temperature.
  • constituents (A) and (B) and also the operating conditions so that this network forms only very partly in aqueous solution.
  • the composition is intended to be applied to the glass-ceramic or the glass to be treated and to form a thin coating by curing or polycondensation through the reaction of the functional groups f (A) of constituent (A) with the functional groups f (B) of constituent (B).
  • the polycondensation product reacts with the glass-ceramic or the glass via SiOH and SiOR radicals, thus making it possible to heal the surface defects thereon, namely checks, cracks, shocks, etc.
  • the film thus formed is intended to improve the mechanical strength of the glass-ceramic or the glass.
  • composition according to the invention may furthermore include:
  • constituent (C1) is or contains a tertiary amine, such as triethanolamine and diethanolamine propanediol.
  • a tertiary amine such as triethanolamine and diethanolamine propanediol.
  • R 5 to R 7 each represent independently, an alkyl or hydroxyalkyl group.
  • the presence of at lea st one catalyst helps to reduce the cure time and the cure temperature, thereby dispensing, in the case of coatings on bottles or the like, with the use of an additional curing oven and making it possible to work at a temperature of the bottles leaving the annealing lehr (for example at 150° C.), as will be described below.
  • the radical polymerization initiators (C2) are, for example, mixtures that include benzophenone, such as Irgacure® 500 sold by Ciba Specialty Chemicals.
  • composition of the invention may furthermore include:
  • waxes mention may be made of polyethylene waxes, whether oxidized or not.
  • the waxes, fatty acid partial esters and fatty acids may be introduced into the composition in the state associated with a surfactant.
  • the protection agents (D) are thermoplastics and possess elastic slip properties. Their inclusion into the thin film formed contributes to scratch/wear protection during use and handling.
  • the polymers in emulsion (E) are in particular chosen from acrylic copolymers in emulsion, such as those of the HYCAR® series sold by Noveon.
  • surfactant (F) mention may be made of polyoxyethylene fatty ethers, such as C 18 H 35 (OCH 2 CH 2 ) 10 OH, known by the name Brij®97, and also polyethylene oxide/polypropylene oxide/polyethylene oxide triblock copolymers. Mention may also be made of the surfactants used in the examples below.
  • composition according to the invention may thus comprise, in aqueous medium, for a total of 100 parts by weight:
  • the subject of the present invention is also a method of treating the glass-ceramic or glass surface in order to improve the mechanical strength thereof by healing the surface defects, characterized in that a thin film of the composition as defined in one of claims 1 to 15 is applied to the glass-ceramic or glass parts to be treated with a thickness that may range up to 3 microns, and in that said composition undergoes a curing or polycondensation reaction.
  • composition according to the invention may be prepared with a view to its application by mixing its constituents, generally at the time of use, in various ways.
  • composition according to the invention contains the constituents (A)+(B)+water
  • it may be prepared by firstly mixing (A) with (B) and then by combining this mixture with water at the time of use.
  • catalysts and/or additives When catalysts and/or additives are present, they may be mixed with the water before (A) is mixed with (B) at the time of use.
  • the composition is applied by spraying or dip coating.
  • the applied coating may undergo a drying operation, for example for a few seconds, followed by passage beneath UV lamps, the UV treatment lasting for example, a few seconds to 30 seconds.
  • the heat curing or polycondensation may be carried out at a temperature of, for example, 100 to 200° C. for 5 to 20 minutes.
  • a temperature for example, 100 to 200° C. for 5 to 20 minutes.
  • the temperature and the duration of the treatment depend on the system used. Thus, there may be systems that allow the thin hard coating to form thermally at room temperature almost instantly.
  • the procedure may be to deposit the composition by spraying it onto the hollowware after the annealing lehr, the temperature of the hollowware during spraying being between 10 and 150° C.;
  • the present invention also relates to a glass-ceramic, flat glass or to hollowware treated by a composition as defined above, according to the method as defined above, and to glass fibers, especially optical fibers (for example those used for dentists' lamps) which are treated by a composition as defined above using the method as defined above.
  • the present invention also relates to the use of a composition as defined above, in order to improve the mechanical strength of the glass-ceramic or the glass by healing its surface defects.
  • Methacryloxypropyltrimethoxysilane 1.5 SR610 600 polyethylene glycol 0.5 diacrylate GK6006 wax 1.5 Surfactant from the family of 0.1 modified polysiloxanes, sold by Byk under the name BYK 341 IRGACURE 500 0.15 Water balance to 100
  • a coating composition for glass was prepared by hydrolyzing the silane of the formulation in water for 24 hours and then by adding the other constituents of the formulation.
  • composition thus obtained was deposited on a batch of 10 flat glass plates (dimensions 70 ⁇ 70 ⁇ 3.8 mm) on which defects were created by a Vickers indenter with a diamond pyramidal tip and an applied force of 50 N.
  • the coating was deposited by dip coating at a controlled rate of 500 mm/min in order to ensure a uniform thickness. This coating operation was carried out 24 hours after the indentation, so as to stabilize the crack propagation and to relax the stresses around the defect created.
  • the glass plates were then dried for 10 minutes at 100° C. and then the film applied as a coating underwent UV curing for 25 seconds, the characteristics of the UV emitter being the following:
  • the fracture test in three-point bending was carried out on the glass plates thus coated, by putting the defect created into extension. This test was performed without UV aging and environmental aging of the coatings formed.
  • a batch of 10 uncoated flat glass plates served as control.
  • the three-point fracture results are expressed as the modulus of rupture (MOR) in MPa and are used to evaluate the reinforcing performance of the composition.
  • the reinforcement results for the coating are expressed as the difference between the modulus of rupture in the bending test for the control flat glass plates and the modulus of rupture of the treated flat glass plates.
  • the graph in FIG. 1 shows the cumulative fracture as a percentage plotted as a function of the modulus of rupture in MPa.
  • the curve showing the 10 coated flat glass specimens is shifted towards higher modulae of rupture compared with the curve for the 10 flat glass specimens with no coating.
  • the coating formed from the composition of this example therefore gives the glass greater mechanical strength.
  • Methacryloxypropyltrimethoxysilane 1 CRAY VALLEY compound 10
  • BYK 3500 UV Copolymeric surfactant sold under the 0.2 name GANTREZ Sodium dodecylsulfate (surfactant) 0.5 Water balance to 100
  • Example 1a For each of the formulations of Examples 1b and 1c, the procedure was as in Example 1a except that the crosslinking time was around 20 seconds.
  • Methacryloxypropyltrimethoxysilane 1 Glycidoxypropylmethyldiethoxysilane 1 GK6006 wax 1.5 Water balance to 100
  • a coating composition for glass was prepared by the following operating method.
  • the two silanes were premixed for 5 minutes and then water was added and the silanes were hydrolyzed with vigorous stirring for 30 minutes. The wax was then added.
  • Example 1b The procedure was then as in Example 1b, except that instead of the drying followed by UV curing, a heat treatment was carried out for 25 minutes at 240° C.
  • Example 1c The same test as in Example 1c was carried out on the glass plates thus coated.
  • Example 3a 3b 3c 3d 3-Aminopropyltriethoxysilane 0.5 1 0.3 0.5 Glycidoxypropylmethyldiethoxysilane 1 2 1 1 OG25 wax 1.5 1.5 1.5 GK6006 wax 1.5 Polyurethane of 25% solids content, 1.5 1.5 1.5 1.5 1.5 sold by Diegel under the name BG49300 Deionized water, balance to 100 100 100 100 100 100
  • a first drum containing the aminopropyltriethoxysilane and the glycidoxypropylmethyldiethoxysilane was prepared by mixing them for 5 to 7 minutes (Example 3a) and for 10 minutes (Examples 3b, 3c and 3d) and, on the other hand, a second drum, containing the polyethylene wax, the polyurethane and the water was prepared, and then the contents of the two drums were mixed together for 30 minutes before application.
  • Example 2b The procedure was then as in Example 2b, except that the heat treatment (curing) was carried out at 200° C. for 20 minutes.
  • Example 1c The same test as in Example 1c was carried out on the glass plates thus coated with the composition of Example 3b.
  • the coating formed from the composition of Example 3b therefore gives the glass greater mechanical strength.
  • the reinforcement provided by the coating based on the composition of Example 3b is unmodified after the WOM and VE aging tests.
  • the glass having the coating based on the composition of Example 3b did not suffer any degradation after 540 hours of UV exposure. It was not impaired by the humidity under the conditions of the VE test described above.
  • Example 4a A composition was prepared as in Example 3a except that both silanes were prehydrolyzed (in Example 4a) and the glycidoxypropylmethyldiethoxysilane was prehydrolyzed (in Example 4b) with all the water for 15 minutes.
  • a composition was prepared as in Example 3a except that 0.15 parts of triethanolamine were added to the second drum (Example 5a).
  • Example 5b A composition was prepared as in Example 3c, except that 0.075 parts of triethanolamine and 0.075 parts of diethanolamine propanediol were added to the second drum (Example 5b).
  • the hydrolysis of the 3-aminopropyltriethoxysilane and the glycidoxypropylmethyldiethoxysilane is completed.
  • the prehydrolysis of the glycidoxypropylmethyldiethoxysilane does not affect the hydrolysis reaction rate of the two silanes.
  • the prehydrolysis of the glycidoxypropylmethyldiethoxysilane does have an influence on the reinforcement over time.
  • One recommended operating method therefore consists in firstly hydrolyzing the glycidoxypropylmethyldiethoxysilane for a few minutes (5 to 10 minutes) in order to achieve a level of reinforcement that is stable and durable.
  • the viscosity of the formulation of Examples 3 and 4 with and without prehydrolysis of the glycidoxypropylmethyldiethoxysilane is dependent on the temperature at which the compound is mixed (20° C. or 40° C.). The viscosity changes more rapidly the higher the temperature.
  • the viscosity of the formulation is also dependent on the nature of the polyethylene wax (OG25 or GK6006) used. When GK6006 is used (Example 3d), the compound seems to be stable over the course of time, whereas when the formulation contains OG25 an increase in viscosity is observed.
  • a more economic use of the curing oven, which is installed in line downstream of the cold end, can be achieved by optimizing the formulation so that it consumes less energy.
  • Defects along the edges are less severe than defects created with a 50 N indenter.
  • the cutting and the shaping of the glass creates smaller defects along the edges.
  • a force of 5 N is applied during the indentation.
  • the size (indentation with 50 N or 5 N) and the nature of the defect (indentation or shaping) lead to different levels of reinforcement for the coating of Example 3a.
  • Table 7 is a table summarizing the results obtained.
  • the glass coating compositions were prepared by the following operating method.
  • the epoxysilane was hydrolyzed for 10 minutes in water and then the aminosilane was added and hydrolyzed for 20 minutes before the GK6006 wax was added.
  • test was carried out on a bottle production line using a 16-section, 32-mold IS machine for 300 and 410 g burgundy bottles.
  • bottles were taken as they left the lehr before the cold treatment and were then treated by spraying them cold under the following conditions: bottles top down on spinners, two nozzles for treating the bottom and sides of the bottles, respectively.
  • the spray nozzles specifically for the sides was 16 cm from the bottle and its spray axis was located at 11 cm from the bottom of this same bottle.
  • the nozzle for the bottom was located at 16 cm from the bottle and it sprayed the sides within 3 cm of the bottom.
  • the rotation speed of the spinner was 120 rpm and the spray times were chosen so as to make complete revolutions.
  • the atomization air pressure was 5.5 bar.
  • Example 11a The parameters were set so as to obtain a spray angle of about 8° with the formulation of Example 11a:
  • bottles removed were treated by spraying (on cold bottles), dried for 15 minutes and then heat treated in an oven for 20 minutes at 200° C.
  • the other bottles served as control.
  • Each series consisted of 320 bottles (10 bottles per mold). The entire surface of the bottles was treated and also the bottom. The thickness of the coating was 150 to 300 nm.
  • the bottles treated with the formulation of Example 10a had a spray angle of 8° while those treated with the formulation of Example lob had a spray angle of 20°.
  • the strength of the bottles was evaluated in an internal pressure test (AGR machine).
  • the burst histograms are given in FIGS. 8 and 9 and the mean burst pressures are given in Table 8 below.
  • Formulation Formulation: Formulation Control Ex. 10b Control Ex. 10a Ex. 10b Mean burst 14.9 ⁇ 0.4 16.6 ⁇ 0.5 22.6 ⁇ 0.8 27.3 ⁇ 1.1 27.4 ⁇ 1.10 pressure Standard 3.5 4.2 7.7 9.4 9.2 deviation % ⁇ 12 bar 19.5 14.5 6.0 1.6 2.8 % ⁇ 15 bar 49.1 34.4 19.4 12.3 11.2
  • Glycidoxypropylmethyldiethoxysilane 1.0 3-Aminopropyltriethoxysilane 0.3 Emulsion of a copolymer having a T g of 2.6 36° C., sold by Noveon under the brand name Hycar ® 26391 Water balance to 100
  • the epoxysilane was dissolved in water for 5 minutes. Then the aminosilane was added and mixed for 15 minutes. Finally, the copolymer emulsion was added and mixed for 3 minutes.
  • the coating compositions thus prepared were deposited on glass specimens indented with 10 N by dipping these glass plates into said compositions at a rate of 50 cm/min, followed by drying the specimens in air for 10 minutes and then heat treating them at 200° C. for 20 minutes.
  • Example 1a The procedure was as in Example 1a, section (c), the results obtained being given in Table 9 below and in FIG. 10 .
  • Example 10a A composition not varying from that of Example 10a except by a GK6006 wax content of 2% instead of 1.5% was sprayed onto a KERABLACK (registered trade mark of Eurokera) glass-ceramic plate.
  • KERABLACK registered trade mark of Eurokera
  • epoxy silane was hydrolyzed for 10 minutes in water and then the aminosilane was added and hydrolyzed for 20 minutes before the GK6006 wax was added.
  • the plates tested were “smooth-smooth”, i.e. both sides being smooth (as opposed to plates mechanically reinforced by forming studs or reliefs on one or both sides, by calendering between rolls having the complementary reliefs). Their dimensions were 300 mm ⁇ 300 mm ⁇ 3 mm (thickness).
  • Spraying was carried out at a rate of 11 l/h and a nozzle displacement speed of 0.45 m/s with 4 translations. A continuous film was formed on one side of the plate, which was dried for 10 minutes in air and then heated for 20 minutes at 200° C.
  • the glass-ceramic plates comply with the domestic electrical appliances standard NF EN-60-335-2-6.
  • the plates were held horizontal so as to leave a 240 mm ⁇ 240 mm central area free, the reinforcing coating according to the invention, when present, being on the underside.
  • the plates were subjected to three series of impacts from above, localized on twelve impact areas according to the NF EN 60-068-2-75 standard (Norwegian hammer).
  • the impact energy of the instrument was 0.7 J.
  • the fracture rates were:
  • Another set of glass-ceramic plates treated according to the invention was subjected to aging over a radiant heat source 145 mm in useful diameter, which was positioned beneath the plates at their center.
  • the coatings of the invention again on the underside, were heated in 450-600° C. cycles for 30 minutes and left to cool down for 30 minutes.

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  • Engineering & Computer Science (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
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  • General Life Sciences & Earth Sciences (AREA)
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  • Crystallography & Structural Chemistry (AREA)
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  • Paints Or Removers (AREA)
  • Surface Treatment Of Glass (AREA)
  • Surface Treatment Of Glass Fibres Or Filaments (AREA)
US11/630,772 2004-07-02 2005-06-15 Composition for treating glass-ceramic or glass to improve mechanical strength through curing of surface defects, treatment methods Abandoned US20090197026A1 (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
FR0407359 2004-07-02
FR0407359A FR2872507B1 (fr) 2004-07-02 2004-07-02 Composition de traitement d'une vitroceramique pour en ameliorer la resistance mecanique par guerison des defauts de surface, procedes de traitement correspondants et vitroceramiques traitees obtenues
PCT/FR2005/050445 WO2006013296A1 (fr) 2004-07-02 2005-06-15 Composition de traitement d'une vitroceramique ou d’un verre pour ameliorer la resistance mecanique par guerison des defauts de surface, procedes de traitement

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US (1) US20090197026A1 (zh)
EP (1) EP1763493A1 (zh)
JP (1) JP5661986B2 (zh)
KR (1) KR101243196B1 (zh)
CN (1) CN1984852A (zh)
FR (1) FR2872507B1 (zh)
WO (1) WO2006013296A1 (zh)

Cited By (4)

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ES2379140A1 (es) * 2010-09-27 2012-04-23 Fundación Investigación E Innovación Para El Desarrollo Social Cerámica de cristal.
WO2013057163A3 (en) * 2011-10-20 2013-08-29 3B Fibreglass Sprl Sizing composition for glass fibres
US11447295B2 (en) 2016-05-12 2022-09-20 Anheuser-Busch Inbev S.A. Glass container having an inkjet printed image and a method for the manufacturing thereof
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EP1763493A1 (fr) 2007-03-21
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